#------------------------------------------------------------------------------ #$Date: 2021-05-22 06:23:35 +0300 (Sat, 22 May 2021) $ #$Revision: 265447 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/06/7060688.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7060688 loop_ _publ_author_name 'Huang, Yao' 'Peng, Ru-Fang' 'Jin, Bo' _publ_section_title ; An efficient strontium-based combustion inhibitor of ammonium perchlorate with a 2D-MOF structure ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D0NJ06239A _journal_year 2021 _chemical_formula_moiety '0.5(C12 H16 N12 O16 Sr2), 2(H2 O)' _chemical_formula_sum 'C6 H12 N6 O10 Sr' _chemical_formula_weight 415.84 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_block_doi 10.5517/ccdc.csd.cc26sc2g _audit_creation_date 2020-12-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-12-09 deposited with the CCDC. 2021-04-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.021(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.7194(9) _cell_length_b 8.3786(7) _cell_length_c 17.7045(15) _cell_measurement_reflns_used 7274 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 27.50 _cell_measurement_theta_min 3.22 _cell_volume 1436.2(2) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_unetI/netI 0.0230 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 10470 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.548 _diffrn_reflns_theta_min 3.215 _exptl_absorpt_coefficient_mu 3.821 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.3640 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1454 before and 0.0508 after correction. The Ratio of minimum to maximum transmission is 0.4882. The \l/2 correction factor is Not present. ; _exptl_crystal_density_diffrn 1.923 _exptl_crystal_description block _exptl_crystal_F_000 832 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.264 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 121 _refine_ls_number_reflns 1661 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.152 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0216 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+1.3510P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0502 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1571 _reflns_number_total 1661 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0nj06239a2.cif _cod_data_source_block ww _cod_database_code 7060688 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.750 _shelx_estimated_absorpt_t_min 0.679 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H,H) groups 2. Restrained distances O1W-H1WB 0.86 with sigma of 0.02 O1W-H1WA 0.86 with sigma of 0.02 H1WB-Sr1 3 with sigma of 0.02 O2W-H2WB 0.86 with sigma of 0.02 O2W-H2WA 0.86 with sigma of 0.02 3.a X=CH2 refined with riding coordinates: N1(H1A,H1B) ; _shelx_res_file ; ww.res created by SHELXL-2014/7 TITL ww_a.res in C2/c REM Old TITL ww in Cc REM SHELXT solution in C2/c REM R1 0.074, Rweak 0.006, Alpha 0.057, Orientation as input REM Formula found by SHELXT: C12 N4 O6 Sr CELL 0.71073 9.7194 8.3786 17.7045 90 95.021 90 ZERR 4 0.0009 0.0007 0.0015 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O Sr UNIT 24 48 24 40 4 DFIX 0.86 O1W H1Wb DFIX 0.86 O1W H1Wa DFIX 3 H1Wb Sr1 DFIX 0.86 O2W H2Wb DFIX 0.86 O2W H2Wa L.S. 4 0 0 PLAN 20 SIZE 0.11 0.1 0.08 TEMP 0 BOND $H list 4 fmap 2 53 acta REM REM REM WGHT 0.019100 1.351000 FVAR 0.38883 SR1 5 0.500000 0.311769 0.750000 10.50000 0.01803 0.01684 = 0.01431 0.00000 0.00274 0.00000 O1 4 0.961013 0.710487 0.536744 11.00000 0.03865 0.03456 = 0.02199 0.00072 0.00873 -0.01623 O1W 4 0.611993 0.549886 0.828583 11.00000 0.03003 0.02929 = 0.02560 -0.00326 0.00583 -0.00311 O2 4 0.689489 0.405489 0.668031 11.00000 0.02765 0.03119 = 0.02488 -0.00177 0.00664 -0.01261 O2W 4 0.571884 0.797288 0.667216 11.00000 0.06849 0.03351 = 0.02659 0.00034 0.01014 -0.01280 O3 4 0.834858 0.567147 0.737349 11.00000 0.02627 0.03094 = 0.01632 -0.00012 0.00131 -0.00747 N1 3 0.693377 0.441927 0.499186 11.00000 0.04735 0.04954 = 0.02154 -0.00063 -0.00440 -0.02431 AFIX 93 H1A 2 0.676024 0.431473 0.450970 11.00000 -1.20000 H1B 2 0.645738 0.389673 0.529597 11.00000 -1.20000 AFIX 0 N2 3 0.872062 0.623453 0.485109 11.00000 0.03597 0.03133 = 0.01910 0.00056 0.00346 -0.00742 N3 3 0.934595 0.674734 0.609181 11.00000 0.02975 0.02886 = 0.01847 0.00074 0.00607 -0.00965 C1 1 0.794213 0.539219 0.526810 11.00000 0.02408 0.02182 = 0.01900 0.00066 0.00192 -0.00093 C2 1 0.835113 0.571874 0.605027 11.00000 0.01952 0.01804 = 0.01779 0.00068 0.00245 -0.00092 C3 1 0.781108 0.508546 0.676110 11.00000 0.01759 0.02056 = 0.01960 0.00232 0.00349 -0.00045 H1WA 2 0.560228 0.630738 0.829065 11.00000 0.05652 H1WB 2 0.686587 0.573743 0.809680 11.00000 0.06402 H2WA 2 0.590775 0.826689 0.623343 11.00000 0.05360 H2WB 2 0.599101 0.875750 0.693084 11.00000 0.06586 HKLF 4 REM ww_a.res in C2/c REM R1 = 0.0216 for 1571 Fo > 4sig(Fo) and 0.0238 for all 1661 data REM 121 parameters refined using 5 restraints END WGHT 0.0191 1.3510 REM Highest difference peak 0.264, deepest hole -0.383, 1-sigma level 0.068 Q1 1 1.1007 0.6648 0.6389 11.00000 0.05 0.26 Q2 1 0.8294 0.5296 0.6379 11.00000 0.05 0.26 Q3 1 0.9884 0.6790 0.6412 11.00000 0.05 0.25 Q4 1 0.6172 1.0366 0.6423 11.00000 0.05 0.23 Q5 1 0.7773 0.7839 0.6960 11.00000 0.05 0.20 Q6 1 0.8255 0.6424 0.8463 11.00000 0.05 0.19 Q7 1 0.8324 0.5227 0.5676 11.00000 0.05 0.18 Q8 1 0.9188 0.5590 0.7270 11.00000 0.05 0.18 Q9 1 0.6784 0.4036 0.7455 11.00000 0.05 0.18 Q10 1 0.7283 0.3521 0.5857 11.00000 0.05 0.17 Q11 1 0.8465 0.3862 0.3964 11.00000 0.05 0.17 Q12 1 0.8542 0.5439 0.5004 11.00000 0.05 0.17 Q13 1 0.8850 0.6214 0.6152 11.00000 0.05 0.17 Q14 1 0.6656 0.3517 0.8457 11.00000 0.05 0.16 Q15 1 0.8579 0.5040 0.7654 11.00000 0.05 0.16 Q16 1 0.7418 0.3545 0.6406 11.00000 0.05 0.16 Q17 1 0.9218 0.4331 0.5849 11.00000 0.05 0.16 Q18 1 0.8657 0.6151 0.7791 11.00000 0.05 0.16 Q19 1 0.6632 0.2732 0.6174 11.00000 0.05 0.16 Q20 1 0.7448 0.4323 0.8596 11.00000 0.05 0.16 ; _shelx_res_checksum 76513 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.5000 0.31177(3) 0.7500 0.01632(8) Uani 1 2 d DS T P . . O1 O 0.96101(15) 0.71049(17) 0.53674(7) 0.0314(3) Uani 1 1 d . . . . . O1W O 0.61199(15) 0.54989(18) 0.82858(8) 0.0281(3) Uani 1 1 d D . . . . O2 O 0.68949(14) 0.40549(16) 0.66803(7) 0.0277(3) Uani 1 1 d . . . . . O2W O 0.5719(2) 0.7973(2) 0.66722(9) 0.0425(4) Uani 1 1 d D . . . . O3 O 0.83486(13) 0.56715(16) 0.73735(7) 0.0245(3) Uani 1 1 d . . . . . N1 N 0.6934(2) 0.4419(2) 0.49919(10) 0.0399(5) Uani 1 1 d . . . . . H1A H 0.6760 0.4315 0.4510 0.048 Uiso 1 1 calc R . . . . H1B H 0.6457 0.3897 0.5296 0.048 Uiso 1 1 calc R . . . . N2 N 0.87206(18) 0.6235(2) 0.48511(9) 0.0287(4) Uani 1 1 d . . . . . N3 N 0.93460(17) 0.67473(19) 0.60918(9) 0.0255(3) Uani 1 1 d . . . . . C1 C 0.79421(19) 0.5392(2) 0.52681(10) 0.0216(4) Uani 1 1 d . . . . . C2 C 0.83511(17) 0.5719(2) 0.60503(10) 0.0184(3) Uani 1 1 d . . . . . C3 C 0.78111(18) 0.5085(2) 0.67611(10) 0.0191(3) Uani 1 1 d . . . . . H1WA H 0.560(3) 0.631(3) 0.8291(16) 0.057(9) Uiso 1 1 d D . . . . H1WB H 0.687(2) 0.574(3) 0.8097(14) 0.064(9) Uiso 1 1 d D . . . . H2WA H 0.591(3) 0.827(3) 0.6233(11) 0.054(8) Uiso 1 1 d D . . . . H2WB H 0.599(3) 0.876(3) 0.6931(16) 0.066(10) Uiso 1 1 d D . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr1 0.01803(12) 0.01684(12) 0.01431(11) 0.000 0.00274(8) 0.000 O1 0.0386(8) 0.0346(8) 0.0220(7) 0.0007(6) 0.0087(6) -0.0162(6) O1W 0.0300(8) 0.0293(8) 0.0256(7) -0.0033(6) 0.0058(6) -0.0031(6) O2 0.0277(7) 0.0312(8) 0.0249(7) -0.0018(6) 0.0066(6) -0.0126(6) O2W 0.0685(12) 0.0335(9) 0.0266(8) 0.0003(7) 0.0101(8) -0.0128(8) O3 0.0263(7) 0.0309(7) 0.0163(6) -0.0001(5) 0.0013(5) -0.0075(6) N1 0.0473(11) 0.0495(12) 0.0215(9) -0.0006(8) -0.0044(8) -0.0243(9) N2 0.0360(9) 0.0313(9) 0.0191(8) 0.0006(7) 0.0035(7) -0.0074(7) N3 0.0298(8) 0.0289(9) 0.0185(7) 0.0007(6) 0.0061(6) -0.0097(7) C1 0.0241(9) 0.0218(9) 0.0190(9) 0.0007(7) 0.0019(7) -0.0009(7) C2 0.0195(8) 0.0180(8) 0.0178(8) 0.0007(7) 0.0024(7) -0.0009(7) C3 0.0176(8) 0.0206(9) 0.0196(8) 0.0023(7) 0.0035(7) -0.0004(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Sr1 O1W 80.53(7) . 2_656 ? O1W Sr1 N3 77.59(5) 2_656 3_445 ? O1W Sr1 N3 147.99(4) 2_656 4_646 ? O1W Sr1 N3 147.99(4) . 3_445 ? O1W Sr1 N3 77.59(5) . 4_646 ? O2 Sr1 O1W 77.37(4) . . ? O2 Sr1 O1W 75.61(5) . 2_656 ? O2 Sr1 O1W 75.61(5) 2_656 . ? O2 Sr1 O1W 77.37(4) 2_656 2_656 ? O2 Sr1 O2 144.36(6) . 2_656 ? O2 Sr1 O3 79.73(4) 2_656 3_445 ? O2 Sr1 O3 79.73(4) . 4_646 ? O2 Sr1 O3 131.35(4) 2_656 4_646 ? O2 Sr1 O3 131.35(4) . 3_445 ? O2 Sr1 N3 74.76(4) . 3_445 ? O2 Sr1 N3 74.76(4) 2_656 4_646 ? O2 Sr1 N3 121.12(5) . 4_646 ? O2 Sr1 N3 121.12(5) 2_656 3_445 ? O3 Sr1 O1W 150.72(4) 3_445 . ? O3 Sr1 O1W 109.30(5) 4_646 . ? O3 Sr1 O1W 150.72(4) 4_646 2_656 ? O3 Sr1 O1W 109.30(5) 3_445 2_656 ? O3 Sr1 O3 75.99(6) 3_445 4_646 ? O3 Sr1 N3 80.91(5) 3_445 4_646 ? O3 Sr1 N3 80.91(5) 4_646 3_445 ? O3 Sr1 N3 60.28(4) 3_445 3_445 ? O3 Sr1 N3 60.28(4) 4_646 4_646 ? N3 Sr1 N3 130.98(7) 3_445 4_646 ? N3 O1 N2 110.00(13) . . ? Sr1 O1W H1WA 113(2) . . ? Sr1 O1W H1WB 107.5(14) . . ? H1WA O1W H1WB 110(3) . . ? C3 O2 Sr1 133.78(11) . . ? H2WA O2W H2WB 101(3) . . ? C3 O3 Sr1 125.94(11) . 3 ? H1A N1 H1B 120.0 . . ? C1 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? C1 N2 O1 105.42(14) . . ? O1 N3 Sr1 135.15(11) . 3 ? C2 N3 Sr1 116.08(11) . 3 ? C2 N3 O1 107.13(15) . . ? N1 C1 C2 127.12(17) . . ? N2 C1 N1 124.40(17) . . ? N2 C1 C2 108.47(16) . . ? N3 C2 C1 108.97(15) . . ? N3 C2 C3 120.16(16) . . ? C1 C2 C3 130.87(16) . . ? O2 C3 O3 127.57(16) . . ? O2 C3 C2 116.71(16) . . ? O3 C3 C2 115.72(15) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O1W 2.6145(14) . ? Sr1 O1W 2.6146(14) 2_656 ? Sr1 O2 2.5656(12) 2_656 ? Sr1 O2 2.5656(12) . ? Sr1 O3 2.6008(13) 4_646 ? Sr1 O3 2.6008(13) 3_445 ? Sr1 N3 2.7678(16) 4_646 ? Sr1 N3 2.7678(16) 3_445 ? O1 N2 1.406(2) . ? O1 N3 1.3631(19) . ? O1W H1WA 0.844(17) . ? O1W H1WB 0.849(17) . ? O2 C3 1.240(2) . ? O2W H2WA 0.850(17) . ? O2W H2WB 0.831(18) . ? O3 Sr1 2.6008(13) 3 ? O3 C3 1.261(2) . ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? N1 C1 1.334(2) . ? N2 C1 1.309(2) . ? N3 Sr1 2.7678(16) 3 ? N3 C2 1.293(2) . ? C1 C2 1.433(2) . ? C2 C3 1.502(2) . ?